CN106146257B - A method of extraction high-purity linalool - Google Patents
A method of extraction high-purity linalool Download PDFInfo
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- CN106146257B CN106146257B CN201610520657.XA CN201610520657A CN106146257B CN 106146257 B CN106146257 B CN 106146257B CN 201610520657 A CN201610520657 A CN 201610520657A CN 106146257 B CN106146257 B CN 106146257B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0223—Moving bed of solid material
- B01D11/0242—Moving bed of solid material in towers, e.g. comprising contacting elements
- B01D11/0249—Moving bed of solid material in towers, e.g. comprising contacting elements comprising jet means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods of extraction high-purity linalool, include the following steps：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, are crushed to 60 80 mesh；The charge door for opening leaching device is 48 by the weight ratio of granular material and solvent:Ethyl alcohol and ethyl acetate mixed solvent is added in 1 proportioning, by conventional filtration, removes residue, obtains crude product；Crude product is put into alembic, is distilled at 75 78 DEG C, slightly fragrant camphor tree essential oil is obtained；Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；It is finally concentrated under reduced pressure in a rotary evaporator, obtains high-purity linalool.This method has many advantages, such as that extraction efficiency is high, product quality is high, simple for process, at low cost, and the yield of linalool reaches 1.8 2.2%, and purity reaches 99.8% or more, and fragrance is good, has good Social benefit and economic benefit, is worthy to be popularized.
Description
Technical field
The present invention relates to technical field of natural plant active ingredient extraction, the side of specifically a kind of extraction high-purity linalool
Method.
Background technology
Camphor tree essential oil is generally colourless or faint yellow oily transparency liquid at normal temperatures, and fractions can analyse at normal temperatures
Go out solid constituent, there is strong special odor, there is stronger volatility, there is higher index of refraction and optical activity mostly；Than
Between focusing on O.86-1.065；It can hardly be dissolved in water, absolute ethyl alcohol can be completely dissolved in, dissolve in the poles such as ether, chloroform, petroleum ether
In the smaller organic solvent of property, volatile decomposition more sensitive to air, light and temperature.
Content is at most linalool also known as Linalool, linalool etc., scientific name 3,7- dimethyl -1,6- in camphor tree essential oil
Octadiene -3- alcohol, chemical formula C10 H18O.Linalool is colourless or light yellow transparent liquid, not soluble in water, can be dissolved in second
Alcohol and ether, have pleasant fragrant and sweet smell, soft aroma and, lightly float hair, is widely used in fragrance, essence, perfume, perfumed soap
In, status is important in monomer perfume, is known as the title of " fragrance U.S. king "；Linalool is the raw material of synthesising complex E again simultaneously, and
Because having the effects that anti-bacteria and anti-virus and analgesia are applied in medicine.
The method that the natural linalool production in China still uses steam distillation at present, since technique is backward and technical conditions
Poor, product yield is low with product quality, and the utilization of resources is extremely insufficient.It is had attracted much attention in current natural perfume material, natural virtue camphor tree
Under the background of alcohol price Continued, the extraction process of linalool is improved, product yield is improved and product quality has become acquisition
High-purity linalool urgent problem to be solved.
Invention content
The present invention for the prior art extraction linalool there are the problem of, provide it is a kind of extraction high-purity linalool side
Method.This method has many advantages, such as that extraction efficiency is high, product quality is high, simple for process, at low cost.
In order to achieve the goal above, the technical solution adopted by the present invention is as follows：
A method of extraction high-purity linalool includes the following steps：
（1）Pretreatment of raw material：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, 60-80 mesh is crushed to, obtains powder
Shape material；
（2）Solvent extraction：The charge door of leaching device is opened, granular material, then the weight by granular material and solvent is added
Amount is than being 4-8:Ethyl alcohol and ethyl acetate mixed solvent is added in 1 proportioning, covers charging lid, closes heater and pumping source, rises
Temperature cycle extraction controls 50-60 DEG C of temperature, and material is discharged from discharge gate in cycle extraction 1-3h, and by conventional filtration, removal is residual
Slag obtains crude product；The cycle extraction is mixed by pumping pressurization, nozzle injection mixing, mixing tube mixes, the reflection of shelves lid mixes,
Tank body flowing mixing and pipeline flow 6 mixed and accelerate extraction mixed zone, strengthen the leaching of active constituent；
（3）Separation：By step（2）Crude product be put into alembic, distilled at 75-78 DEG C, recycle mixed solvent, obtain slightly
Fragrant camphor tree essential oil；
（4）Removal of impurities：Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；
（5）It is concentrated under reduced pressure：By step（4）Extract be concentrated under reduced pressure in a rotary evaporator, control vacuum degree in 0.08-
0.09Mpa, temperature are evaporated at 50-60 DEG C, obtain high-purity linalool.
Preferably, the weight ratio of ethyl alcohol and ethyl acetate described above is 2-3:1.
Preferably, above step（2）The leaching device includes extractor, mixing tube and pump, and the mixing tube is to pass through
Mixing tube supporting rod is fixed on the central axes of extractor, and the capping of one end of the extractor is equipped with nozzle, extractor it is another
End is equipped with door, and the door is fixed on by door supporting rod in the capping of extractor, and the nozzle is by being equipped with heater
Circulation pipe be connected to the discharge port of pump, the feed inlet of the pump is connected by the another port of circulation pipe and extractor, described
The top of extractor is equipped with charge door, and the bottom of extractor is additionally provided with discharge gate.
Preferably, mixing tube described above be inside spin tube body, mixing tube one end of corresponding nozzle be equipped with it is tubaeform into
Material mouth.
Preferably, extractor described above is additionally provided with temperature measuring set.
The purity of linalool described above reaches 99.8% or more.
Compared with prior art, beneficial effects of the present invention are：
1, the method for the present invention not only increases the yield of linalool, entirely using the essential oil of solvent method extraction Cinnamomum camphora leaves
Extraction process temperature is relatively low, not only consumes energy low and of low cost, additionally it is possible to prevent temperature is excessively high from linalool being caused to be become by thermal oxide
Matter improves the quality of linalool product, overcomes that there are product yields is low with poor product quality using steam distillation
Problem.
2, the method for the present invention uses ethyl alcohol and ethyl acetate mixed solvent as extractant, compared with single alcohol solvent,
The recovery rate of linalool improves 20% or so.
3, the leaching device used in the method for the present invention is mixed by designing pump pressurization, nozzle sprays mixing, mixing tube mixes,
6 of shelves lid reflection mixing, tank body flowing mixing and pipeline flowing mixing accelerate extraction mixed zone so that camphortree leaf powder material
It can adequately be collided with solvent, infiltration of the solvent to camphor tree leaf cell film, camphor tree essential oil accelerated to be easier from intracellular release
Out, material and solvent constantly recoil flowing, are more advantageous to solutes accumulation, improve the oil yield of essential oil, can reach ultrasonic wave
Extraction effect, but equipment cost is lower, is more suitable for industrialized production.
4, the yield of the method for the present invention linalool reaches 1.8-2.2%, and purity reaches 99.8% or more, and fragrance is good, has good
Good Social benefit and economic benefit, is worthy to be popularized.
Description of the drawings
Fig. 1 is the process flow chart of present invention extraction high-purity linalool；
Fig. 2 is the structural schematic diagram of leaching device.
In reference numeral, 1- doors, 2- extractors, 3- mixing tubes, 3a- mixing tube feed inlets, 3b- mixing tube supporting rods,
4- discharge gates, 5- heaters, 6- pumps, 7- circulation pipes, 8- nozzles, 9- charge doors, the filler 10-, 11- temperature measuring sets, 12- pressures
Power table, 13- safety valves.
Specific implementation mode
Below in conjunction with embodiment and attached drawing, the present invention is further described, but is not limited to protection scope of the present invention.
As shown in Fig. 2, leaching device as described below, including extractor 2, mixing tube 3, pump 6 and charge door 9, it is described mixed
Closing pipe 3 is fixed on the central axes of extractor 2 by mixing tube supporting rod 3b, and one end capping of the extractor 2 is equipped with spray
The other end of mouth 8, extractor 2 is equipped with door 1, and the door 1 is fixed on by door supporting rod 1a in the capping of extractor 2,
The nozzle 8 is connected to by the circulation pipe 7 equipped with heater 5 with the discharge port of pump 6, and the feed inlet of the pump 6 passes through circulation pipe 7
It is connect with the another port of extractor 2, the top of the extractor 2 is equipped with charge door 9, and the bottom of extractor 2 is additionally provided with discharge
Mouth 4.The extractor 2 is additionally provided with temperature measuring set 11.Filler is equipped between the top and circulation pipe 7 of the extractor 2
10.2 top of the extractor is additionally provided with pressure gauge 12 and safety valve 13.The charge door is covered equipped with fast-open type.The mixing
Pipe 3 is inside spin tube body, and mixing tube 3 is equipped with tubaeform feed inlet in one end of corresponding nozzle 8.
Embodiment 1
A method of extraction high-purity linalool includes the following steps：
（1）Pretreatment of raw material：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, 60 mesh is crushed to, obtains powdery
Material；
（2）Solvent extraction：The charge door of leaching device is opened, 100kg granular materials are added, then press granular material and solvent
Weight ratio be 6:(weight ratio of ethyl alcohol and ethyl acetate is 2 for 1 proportioning addition ethyl alcohol and ethyl acetate mixed solvent：1）, cover
Feed lid, closes heater and pumping source, and ramp cycle extraction controls temperature 50 C, and cycle extraction 2h is discharged from discharge gate
Material removes residue, obtains crude product by conventional filtration；Pump pressurization mixing is passed through in the cycle extraction, nozzle injection mixes,
6 of mixing tube mixing, shelves lid reflection mixing, tank body flowing mixing and pipeline flowing mixing accelerate extraction mixed zone, strengthen and live
The leaching of property ingredient；
（3）Separation：By step（2）Crude product be put into alembic, distilled at 75 DEG C, recycle mixed solvent, obtained slightly fragrant
Camphor tree essential oil；
（4）Removal of impurities：Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；
（5）It is concentrated under reduced pressure：By step（4）Extract be concentrated under reduced pressure in a rotary evaporator, control vacuum degree exist
0.09Mpa, temperature are evaporated at 50 DEG C, obtain high-purity linalool 2.1kg.
Linalool is qualitatively and quantitatively analyzed using GC, GC-MS, the content of linalool is 99.86%.
Embodiment 2
A method of extraction high-purity linalool includes the following steps：
（1）Pretreatment of raw material：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, 60 mesh is crushed to, obtains powdery
Material；
（2）Solvent extraction：The charge door of leaching device is opened, 100kg granular materials are added, then press granular material and solvent
Weight ratio be 5:(weight ratio of ethyl alcohol and ethyl acetate is 3 for 1 proportioning addition ethyl alcohol and ethyl acetate mixed solvent：1）, cover
Feed lid, closes heater and pumping source, and ramp cycle extraction controls temperature 60 C, and cycle extraction 1h is discharged from discharge gate
Material removes residue, obtains crude product by conventional filtration；Pump pressurization mixing is passed through in the cycle extraction, nozzle injection mixes,
6 of mixing tube mixing, shelves lid reflection mixing, tank body flowing mixing and pipeline flowing mixing accelerate extraction mixed zone, strengthen and live
The leaching of property ingredient；
（3）Separation：By step（2）Crude product be put into alembic, distilled at 78 DEG C, recycle mixed solvent, obtained slightly fragrant
Camphor tree essential oil；
（4）Removal of impurities：Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；
（5）It is concentrated under reduced pressure：By step（4）Extract be concentrated under reduced pressure in a rotary evaporator, control vacuum degree exist
0.08Mpa, temperature are evaporated at 55 DEG C, obtain high-purity linalool 1.8kg.
Linalool is qualitatively and quantitatively analyzed using GC, GC-MS, the content of linalool is 99.90%.
Embodiment 3
A method of extraction high-purity linalool includes the following steps：
（1）Pretreatment of raw material：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, 80 mesh is crushed to, obtains powder
Material；
（2）Solvent extraction：The charge door of leaching device is opened, 100kg granular materials are added, then press granular material and solvent
Weight ratio be 4:(weight ratio of ethyl alcohol and ethyl acetate is 2 for 1 proportioning addition ethyl alcohol and ethyl acetate mixed solvent：1）, cover
Feed lid, closes heater and pumping source, and ramp cycle extraction controls temperature 50 C, and cycle extraction 3h is discharged from discharge gate
Material removes residue, obtains crude product by conventional filtration；Pump pressurization mixing is passed through in the cycle extraction, nozzle injection mixes,
6 of mixing tube mixing, shelves lid reflection mixing, tank body flowing mixing and pipeline flowing mixing accelerate extraction mixed zone, strengthen and live
The leaching of property ingredient；
（3）Separation：By step（2）Crude product be put into alembic, distilled at 78 DEG C, recycle mixed solvent, obtained slightly fragrant
Camphor tree essential oil；
（4）Removal of impurities：Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；
（5）It is concentrated under reduced pressure：By step（4）Extract be concentrated under reduced pressure in a rotary evaporator, control vacuum degree exist
0.08Mpa, temperature are evaporated at 60 DEG C, obtain high-purity linalool 2.2kg.
Linalool is qualitatively and quantitatively analyzed using GC, GC-MS, the content of linalool is 99.92%.
Claims (4)
1. a kind of method of extraction high-purity linalool, it is characterised in that：Include the following steps：
(1) pretreatment of raw material：Fresh Cinnamomum camphora leaves are subjected to vacuum freeze drying processing, 60-80 mesh is crushed to, obtains powder
Material；
(2) solvent extraction：The charge door of leaching device is opened, granular material, then the weight ratio by granular material and solvent is added
For 4-8:Ethyl alcohol and ethyl acetate mixed solvent is added in 1 proportioning, covers charging lid, closes heater and pumping source, heating follows
Ring extracts, and controls 50-60 DEG C of temperature, and cycle extraction 1-3h is discharged material from discharge gate, by conventional filtration, removes residue, obtain
Crude product；The cycle extraction is by pump pressurization mixing, nozzle injection mixing, mixing tube mixing, shelves lid reflection mixing, tank body stream
Dynamic mixing and pipeline flow 6 mixed and accelerate extraction mixed zone, strengthen the leaching of active constituent；
(3) it detaches：The crude product of step (2) is put into alembic, is distilled at 75-78 DEG C, mixed solvent is recycled, obtains slightly fragrant camphor tree
Essential oil；
(4) it cleans：Thick fragrant camphor tree essential oil is dried by anhydrous sodium sulfate, then passes through conventional filtering, obtains extract；
(5) it is concentrated under reduced pressure：The extract of step (4) is concentrated under reduced pressure in a rotary evaporator, control vacuum degree is in 0.08-
0.09Mpa, temperature are evaporated at 50-60 DEG C, obtain the high-purity linalool that purity reaches 99.8% or more；
Step (2) described leaching device includes extractor, mixing tube and pump, and the mixing tube is fixed by mixing tube supporting rod
On the central axes of extractor, one end capping of the extractor is equipped with nozzle, and the other end of extractor is equipped with door, the gear
Lid is fixed on by door supporting rod in the capping of extractor, the discharging that the nozzle passes through circulation pipe and pump equipped with heater
The feed inlet of mouth connection, the pump is connected by the another port of circulation pipe and extractor, and the top of the extractor, which is equipped with, to be added
The bottom of material mouth, extractor is additionally provided with discharge gate.
2. the method for extracting high-purity linalool according to claim 1, it is characterised in that：The ethyl alcohol and ethyl acetate
Weight ratio is 2-3:1.
3. the method for the extraction high-purity linalool according to claim 1, it is characterised in that：The mixing tube is interior spiral shell
Coil body, mixing tube are equipped with tubaeform feed inlet in one end of corresponding nozzle.
4. the method for the extraction high-purity linalool according to claim 1, it is characterised in that：The extractor is additionally provided with
Temperature measuring set.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106699515A (en) * | 2016-12-07 | 2017-05-24 | 广西灏源盛世生物科技有限公司 | Method for extracting linalool from ho leaves |
| CN111701273A (en) * | 2020-07-03 | 2020-09-25 | 山东冰文生物技术有限公司 | Alcohol precipitation device is used in production of acid chondroitin |
| CN112262857B (en) * | 2020-10-23 | 2021-10-08 | 珍田(泉州)生物科技有限公司 | Soil purifying agent for preventing and treating root-knot nematode |
| CN113185381A (en) * | 2021-04-20 | 2021-07-30 | 金溪华香香料有限公司 | Method for separating and extracting linalool by taking camphor tree leaves as raw materials through high-speed countercurrent chromatography |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272824A (en) * | 2015-11-17 | 2016-01-27 | 鹰潭华宝香精香料有限公司 | Preparation method of natural cinnamomum camphora aromatic material |
| CN205235459U (en) * | 2015-12-10 | 2016-05-18 | 冯文静 | Natural products active ingredient's pressurization reverse cycle extraction element |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272824A (en) * | 2015-11-17 | 2016-01-27 | 鹰潭华宝香精香料有限公司 | Preparation method of natural cinnamomum camphora aromatic material |
| CN205235459U (en) * | 2015-12-10 | 2016-05-18 | 冯文静 | Natural products active ingredient's pressurization reverse cycle extraction element |
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